South African Journal of Chemical Engineering 43 (2023) 266–272
Available online 17 November 2022
1026-9185/© 2022 The Authors. Published by Elsevier B.V. on behalf of Institution of Chemical Engineers. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Filter material based on zeolite-activated charcoal from cocoa shells as ammonium adsorbent in greywater treatment
Susilawati
a,*, Yuan Alfinsyah Sihombing
a, Siti Utari Rahayu
a, Yuni Yati Br Sembiring
a, Lilik Waldiansyah
a, Mutia Irma
baDepartment of Physics, Faculty of Mathematics and Natural Sciences, Universitas Sumatera Utara, Medan, 20155, Indonesia
bIntegrated Research Labolatory, Universitas Sumatera Utara, Medan, 20155, Indonesia
A R T I C L E I N F O Keywords:
Natural zeolite Activated charcoal Wastewater treatment Adsorption, Ammonium removal
A B S T R A C T
A filter based on zeolite-activated charcoal cocoa shells has been made as an ammonium absorber in greywater.
The two filter materials, Zeolite as matrix and activated charcoal of cocoa shells as filler, were first prepared in powder form with a size of 75 µm (200 mesh). The zeolite matrix was chemically activated using 1 M NaCl solution and dried at 100 ◦C for 24 h, while the activated charcoal filler of cocoa shell was carbonized at 150◦C for 1 hour. The filters were printed using a hydraulic press with a given mass of 5 tons for 10 min, with variations in the composition of zeolite and activated charcoal cocoa shell in the filter, namely (75:25)%, (80:20)%, (85:15)%, (90:10)%, (95:5)%, (100:0)%. The filters were then physically activated with sintering process at temperature variations of 700 ◦C, 800 ◦C, and 900 ◦C, for 4 h. The physical and mechanical properties of the filters were characterized to determine the value of porosity, water absorption and hardness of the filters. Filter with the optimum physical test was found in the sample with the composition of (75:25)% which is sintered at a temperature of 700 ◦C. This filter is known to have with a porosity value of 53.01%, water absorption capacity of 53.10%. Meanwhile, the filter with the best hardness value was found in the sample with a composition of (100:0)% which was sintered at a temperature of 900◦C with a value of 351.31 MPa. The test application of the filter as an ammonium absorber revealed that the filter was capable to reduce the ammonium concentration in greywater treatment up to 75.95%.
1. Introduction
Domestic waste is known to be one of the causes of a decrease in environmental quality (Firdayati et al., 2015; Khalid et al., 2018).
Greywater is a type of domestic which can be a significant source of water pollution due to the large quantity and lack of treatment (Boano et al., 2020; Edwin et al., 2014). Furthermore, the nitrogen content in greywater has the potential to form ammonia compounds (NH3), which will form ammonium ions (NH4+) at low pH (acidic) (Lin et al., 2013;
Oteng-Peprah et al., 2018; Widiastuti et al., 2011). Ammonia can be toxic to humans in amounts that exceed the maximum limit that the body can detoxify. The serious risk of ammonia poisoning is irritation of the skin, eyes, and respiratory tract. Ammonia poisoning can be fatal at extremely high levels (Murphy, 2007; Rakesh et al., 2020). Worse, if the concentration of dissolved ammonia in the water rises, almost all aquatic organisms can become poisoned (Hargreaves J. A., 2004;
Hlordzi et al., 2020). As a result, efforts must be made to reduce the
concentration of dissolved ammonium in greywater in order to maintain a safe ecosystem and environment for living things.
The removal of ammonium from wastewaters and other point sour- ces has thus been accomplished using a variety of techniques, including biological, physical, chemical, or a combination technique. They mainly include ion exchange and adsorption, biological technology, air strip- ping, breakpoint chlorination, chemical precipitation, reverse osmosis, microwave radiation, and supercritical water oxidation. The advantages and disadvantages of these technologies have been researched, there are several limitations of the current technologies, including high cost, low removal rate, high sensitivity to pH and temperature, and introducing new pollutants. Compared to other techniques, ion exchange and adsorption technique have many favourable characteristics (Amiri et al., 2019; Guˇstin and Marinˇsek-Logar, 2011; Huang et al., 2015; Turan, 2016). It demonstrates a high affinity towards ammonium, high removal efficiency, low-cost, simplicity of application and operation as well as environmental friendliness (Amiri et al., 2019; Turan, 2016; Uurlu and
* Corresponding author.
E-mail address: [email protected] (Susilawati).
Contents lists available at ScienceDirect
South African Journal of Chemical Engineering
journal homepage: www.elsevier.com/locate/sajce
https://doi.org/10.1016/j.sajce.2022.11.006
Received 12 May 2022; Received in revised form 21 August 2022; Accepted 14 November 2022
South African Journal of Chemical Engineering 43 (2023) 266–272 Karaolu, 2011; Widiastuti et al., 2011). These advantages make it
competitive to apply on a large scale for commercial and water treat- ment plants to remove ammonium particularly for greywater.
The use of zeolite as an ammonium adsorber material in greywater requires special consideration in this effort because zeolite has been studied as an adsorber material for long time (Hargreaves J. A., 2004;
Hlordzi et al., 2020; Widiastuti et al., 2011). Zeolite has the potential to be used as an adsorber because it has a regular amorphous structure with interconnected cavities in all directions, the ability to absorb small molecules, and a very large zeolite surface area (Kim and Ahn, 2012; Shi et al., 2017). According to the literature studies that have been con- ducted, the use of zeolite as a filter material has been widely used, particularly in its application to absorb water (de Magalh˜aes et al., 2022;
Shi et al., 2017; Widiastuti et al., 2011; Zhang et al., 2019). However, there are different types of zeolites in nature, each with its own set of characteristics (Krol, 2020; ´ Sobu´s et al., 2020; Stocker et al., 2017).
Natural zeolite from Pahae, North Sumatra, has been reported to absorb water vapor by 48.05% at 60 Mesh size and 68.05% at 200 Mesh size higher than natural zeolite from Cikalong (Nasution et al., 2015). This is also supported by previous research which reported that ethanol puri- fication using 200 mesh size natural zeolite was able to absorb 53.82%
of water, and it was shown to increase the ethanol concentration from 90% to 93.28% with a contact time of 60 min (Susilawati et al., 2018).
Therefore, pahae natural zeolite can be promoted as an adsorbent ma- terial for high adsorption rates (Nasution et al., 2015).
Literature studies were also carried out to study the potential of zeolite selectively for ammonia absorption. Several studies have found that the modification of Yemeni natural zeolite with a size of 200–300 mesh that was chemically activated with 1 mol/L NaCl solution while physically activated with stirring for 1 hour at 80 ◦C produced ammo- nium filtration material with high selectivity, because it can absorb 99%
dissolved ammonium (NH4+) (Susilawati et al., 2018). Another study also found that acid-modified Bayah’s natural zeolite was effective in lowering the concentration of dissolved ammonium in milkfish ponds.
The results of this study revealed that using chemically activated zeolite for 30 min with a 1 M HCl solution reduced the ammonium concen- tration in the pond by 92.99% (Susilawati et al., 2020).
To optimize the use of zeolite as a filtration material, particularly as a filter that can selectively absorb ammonia, other materials must be added to optimize the role of the filter, such as material with high adsorption capabilities i.e. activated charcoal. Cocoa shells was chosen because it was found plentiful cocoa plantations in Indonesia and is a waste product from cocoa pods. Besides, the use of cocoa pod waste has a high potential for pectin production, due to the structure of the pectin component contains many active groups, pectin can be used as a bio- adsorber source (Hennessey-Ramos et al., 2021; Njoku, 2014). Previous research, which investigated the production of filter material from clay and cocoa activated carbon powder with various compositions, revealed that the optimum composition for use as a filter material for variations in the composition of clay and cocoa shell powder (65:35)%, with a sin- tering temperature of 320 ◦C has a water absorption value ranging from 86%, a density of 0.322 gr/cm3 and a porosity of 52,38%, successfully filtered water that already met the standard of clean water (Hennes- sey-Ramos et al., 2021; Njoku, 2014).
According to the literature review, there are no published studies that report the production of filters using a combination of zeolite-based materials and activated charcoal from cocoa shells. As a result, this research focus on explored the possibility of employing zeolite-based materials and activated charcoal from cocoa shells as an ammonium absorber in greywater.
2. Materials and methods 2.1. Materials
Pahae natural zeolite was collected from the Pahae District of North
Tapanuli, North Sumatra, Indonesia. The cocoa shells used in this study was obtained from Sayum Sabah village in the Sibolangit district of North Sumatra. Greywater was sampled from a laundry facility near the Universitas Sumatera Utara, Medan, Indonesia.
2.2. Zeolite preparation
The zeolite, which was still in lump form, was first crushed and ground with a mortar and pestle. Ground zeolite was then sieved through a 200 mesh sieve, washed three times with distilled water, and dried in an oven for 24 h at 100 ◦C. The zeolite was then chemically activated for 1 hour in 1 M NaCl solution while stirring with a magnetic stirrer at 135 rpm at 80 ◦C. The chemically activated Pahae zeolite was then re-dried in an oven at 100 ◦C for 24 h. Finally, the dried Pahae Zeolite was ready for use.
2.3. Activated carbon preparation
The cocoa shells were used in this study was a yellow (ripe) cocoa shells from Sayum Sabah village, Sibolangit district, North Sumatra. The collected cocoa shells were cleaned of any remaining seeds and fruit flesh before were cutted into small pieces and dried openly under the sunlight. After drying, the cocoa shells were carbonized in a furnace at 150 ◦C for 1 hour in a neutral atmosphere to produce activated charcoal.
Once it has become activated carbon, the cocoa shells were crushed using a mortar then sieved using a 200 mesh (75 µm) sieve. Cocoa shell activated carbon that has complied with SNI No.06–3730–1995 is now ready to be used.
2.4. Zeolite-cocoa shells activated carbon filter manufacture
The filter was made by combining and sintering zeolite and activated charcoal from cocoa shells. These two ingredients were stirred for 5 min in a 550 cc YM1832 Yami shaker with variations in composition, of (100:0)%, (95:5)%, (90:10)%, (85:15)%, (80:20)%, (75:25)% wt. 50%
v/w of distilled water then added to the mixture and the stirred were continued several times more. The samples were then molded for 10 min on a Hydraulic Press Ytd27–200t with a 5 tons mass. The printing pro- cedure was then repeated for the remaining composition samples. To avoid the cracking during physical activation by heating, the sample was left for 1 week in the open air before the sintering process. After 1 week, the samples are ready to be physically activated for 4 h at temperatures of 700 ◦C, 800 ◦C, and 900 ◦C.
2.5. Porosity test
Due to the porosity features affect the absorption capacity of the sample, porosity testing was done to identify how many pores were present in each sample. According to Eq. (1), the porosity value was defined as the ratio between the total volume of a sample and the number of pore volumes (volume of empty space) in the sample.
%porosity=
(mw− md
ρw×Vt
)
× 100% (1)
Where: mw=wet mass (g); md=dry mass (g); ρw=density of water (g/
m3); Vt =sample volume after burning (m3) 2.6. Water absorption test
The water absorption capacity test of each sample can be assessed by weighing the dry mass and wet mass of the sample. The dry mass is the weight of the sample when it is dry, whereas the wet mass is the weight of the sample after it has been immersed in water for 24 h at room temperature. Eq. (2) can be used to calculate the value of water absorption.
Susilawati et al.
%water absorption test=
(mw− md
md
)
× 100% (2)
Where: mw=wet mass (g); md=dry mass (g) 2.7. Hardness test
The resistance of a substance to plastic deformation caused by pressure or scratching is known as hardness. The Vickers Hardness tool is used to determine the hardness of the material. Eq. (3) is then used to calculate the hardness value.
Hv =1,8544F
d2 (3)
Where: Hv =Hardness of Vickers (MPa); F =given load (N); d =sample diagonal length (m)
2.8. Ammonium removal efficiency
Greywater was collected and stored at 4 ◦C before further used. The greywater was then diluted using distilled water in order to obtain several levels of ammonium concentration. The batch experiments were carried out by shaking a Zeolite-cocoa shells activated carbon filter with 100 mL leachate solution at 180 rpm. Effluent samples were taken after batch experiment. Ammonium concentration remained in effluent so- lution was then determined using UV–Vis spectroscopy under (APHA, 1998) method. The percentage of ammonium removal efficiency from the greywater was then calculated using Eq. (4).
Removal Efficiency(%) =Co− Ce
Co
× 100% (4)
Where: Co =initial ammonium concentration (mg/L); Ce =equilibrium ammonium concentration (mg/L).
2.9. Statistical analysis
STATISTICA 13.0 (StatSoft) software was used to do the calculations.
3. Results and discussion 3.1. Porosity analysis
Natural plant fiber, cocoa shells, can be directly carbonized without
melting to produce carbon fibers and activated carbon fibers (Yue and Economy, 2017). The carbonized process conducted in range 150–240 ◦C that Splitting up of the structural water occurs from hydrogen and hydroxyl fragments present. C––O and C––C bonds form, and the dehydration process is essentially intramolecular. Furthermore, Physical activation develops porosity by the selective gasification of carbon with oxidizing gas at 500–1200 ◦C, Meanwhile in this study conducted on 700, 800 and 900 ◦C. The removal of carbon atoms creates pores, increases the average size of the micropores already accessible to the gas, and opens up closed pores that are created during carbonization (Yue and Economy, 2017). Base on that data, the activated carbon preparation process in this study was in accordance with the protocols, and the activated charcoal produced from cocoa shells met the re- quirements. Thus, that the material can be classified as activated charcoal.
The porosity value of cocoa shells activated charcoal is 58.73%.
Fig. 1 shows that the sample with a composition of (75:25)% that was activated at a temperature of 700 ◦C has the highest porosity value of 53.01%, while the sample with a pure zeolite composition ((100: 0)%) that was activated at a temperature of 700 ◦C has a smaller porosity of 23.80%. Thus, the addition of cocoa shells activated charcoal filler in the sample is known to be able to increase the porosity of the filter due to.
The activation temperature used is also known to greatly affect the porosity value, since the higher the temperature used in the activation process, the denser the pore diameter in the sample. Moreover, based on the porosity test graph observations, it can be seen that the samples activated at a temperature of 900 ◦C tend to have a flat curve. This happens due to the number of pore distributions in the sample decreases.
3.2. Water absorption analysis
Fig. 2. demonstrates that the sample with a composition of (75:15)%
activated at 700 ◦C has the maximum water absorption capacity of 53.10%, whereas the filter with a zeolite composition of only (100: 0)%
active at 700 ◦C has a reduced water absorption capacity of 29.75%. The use of cocoa shell activated charcoal filler in the filter is known to in- crease the water absorption value, according to the results of the anal- ysis. The water absorption value produced is directly proportional to the porosity value, where it can be analyzed that the larger the pores or cavities of a zeolite, the higher the water absorption value.
The value of water absorption is also known to be affected by acti- vation temperature. The lower the water absorption value, the higher the activation temperature employed. This is due to the fact that the higher the temperature at which the filter is activated, the smaller the pore diameter will be formed. Based on the test results, filters with an Fig. 1. Porosity test graph of the filters (n =5).
Fig. 2. Water absorption graph of the filters (n =5).
South African Journal of Chemical Engineering 43 (2023) 266–272
activation temperature of 900 ◦C was analyzed tend to have a flat graph trend. This is due to the smaller pore distribution due to the high tem- perature increase.
3.3. Hardness analysis
The results of the hardness test on a zeolite-based filter, activated charcoal, and cocoa shell are plotted in Fig. 3 From the figure, it can be seen that the highest hardness was obtained in the sample with a composition of (100: 0)% which was activated at a temperature of 900 ◦C with a hardness value of 351.31 MPa. Meanwhile, samples with a composition of (100:0)% which were activated at 800 ◦C and 700 ◦C had hardness value of 253.06 MPa and 205.10 MPa, respectively. Based on the results of the analysis carried out, it is known that the higher the activation temperature used, the higher the hardness value of the sam- ple. This is because the smaller and denser the pore diameters of the filter are the higher the activation temperature employed in combustion.
Meanwhile, the hardness value was recognized to have no significant correlation with the material composition in the filter. The main factor that affects the value of filter hardness is the sintering temperature of the zeolite and activated charcoal of cocoa shells (Susilawati et al., 2021).
This is in accordance with previous studies that used clay and cocoa shell powder with several variations in composition in making filters whose sintering temperature varied from 200 to 320 ◦C. The results of the study showed that the optimum composition to be used as a filter material is the filter with a composition of (65:35)% with a sintering temperature treatment of 320 ◦C (Susilawati et al., 2020), its related with this study where the zeolite has a sintering temperature of around 400–900 ◦C and the optimum hardness value is found on samples with a sintering tem- perature of 900 ◦C.
Fig. 3. Hardness graph of the filters (n =5).
Fig. 4.SEM images of filters which sintered at a temperature of 700 ◦C with a percentage variation composition of (a) 100:0; (b) 95:5; (c) 90:10; (d) 85:15; (e) 80:20 and (f) 75:25.
Susilawati et al.
3.4. Morphological analysis
The morphological test revealed that the five variations in the composition of the materials contained in the filter had not been mixed evenly. This can be seen from the pore diameters on the filters surface on Fig. 4. The results of the pore diameter on variations in material composition, namely composition (100:0)%, (95:5)%, (90:10)%, (85:15)%, (80:20)%, (75:25)% have an average diameter of mean d = 6347 m, 4965 m, 4884 m, 5055 m, 4193 m, 3267 m, respectively. Ac- cording to the results of the SEM test analysis of the five variations in the composition of the material on the filter compared to the pure zeolite sample, the addition of cocoa shell activated charcoal filler affects the diameter of the filter pores. It can be seen that the more activated charcoal used, the smaller the pore size of the filter.
3.5. EDX analysis
The addition of cocoa shell activated charcoal to the filter during manufacturing process aims to optimize the use of the filter as an adsorber. The EDX test was carried out to determine the elemental content in the filter that affects the adsorption capacity of the filter surface.
The basic constituents of zeolite are silicon, aluminum, and oxygen, and it binds a specific quantity of water molecules in its pores. This is shown by the results of the EDX test on the filter as shown in Fig. 5(a).
The percentages of numerous major components in zeolite, including as O2, Si, Al, and Si/Al, are 67.97%, 31.87%, 9.03%, and 3.52%, respec- tively. According to Fig. 4(b), cocoa shells activated charcoal contains numerous dominating components, including O (Oxygen) and K
(Potassium), which account for 33.97 and 5.56% of the total, respec- tively. However, according to the analysis results, Si element is absent.
Fig. 5(g). depicts a compound in the filter with a composition of (75:25)%, namely: O (Oxygen) 54.88%, Si (Silica) 28.63%, Al (Aluminum) 7.75% and Si/Al ratio in the filter is 3.69. It was related to a previous study that discovered that the greater the number of O ele- ments in the filter, the more cavities form on the filter’s surface. As a result, the filter absorbs more water vapor and produces more high- quality hydrogen. Whereas the more Si elements in the filter, the stronger the Si bonds with O, resulting in a harder hydrogen filter than a pure zeolite hydrogen filter (Susilawati et al., 2021).
Based on the elemental composition shown in Fig. 5, it is clear that the zeolite sample contains more oxygen elements than the other ele- ments in all samples, indicating that the sample has uniform pores.
Furthermore, it is known that impurities such as ferum, potassium, calcium, sodium, and magnesium exist in each sample and have a negative impact on the filter because they can reduce the maximum adsorption potential of the zeolite by closing the pores on the zeolite surface.
According to the test results, the Si/Al ratio in the zeolite matrix is 3.52. Based on the Si/Al ratio, the zeolite in this study is classified as a modernite zeolite with an intermediate absorption capacity. The reduction of Al content in zeolite indicates that the zeolite experienced a dealumination process. The more hydrophilic the zeolite, the lower the Si/Al ratio (Sentosa et al., 2018). The greater the Si/Al ratio, the lower the Al content of the zeolite.
Fig. 5. EDX test results of samples at sintering temperature of 700 ◦C. (a) zeolite matrix; (b) activated carbon; filter with a percentage variation composition of (c) 95:5; (d) 90:10; (e) 85:15%; (f) 80:20; and (g) 75:25.
South African Journal of Chemical Engineering 43 (2023) 266–272
3.6. X-ray diffraction (XRD) analysis
The purpose of X-Ray Diffraction (XRD) analysis of non-activated and activated natural zeolite particles is to determine the crystal struc- ture contained in the natural zeolite particles via a graph of the rela- tionship between counts and position (2θ), which means that the greater the intensity that appears, the higher the level of crystanillity in a material.
The mordenite phase is represented in the image by the composition of the (100:0)% zeolite matrix, with peaks of 2θ =28.0383 and 2θ = 29.8466. According to previous research, non-activated 325 mesh zeolite contains mordenite phase at 2θ = 25–30⁰ (Susilawati et al., 2021). In this study, it is expected that the presence of filler will increase the intensity of the filter. However, the resulting diffraction pattern in all compositions in Fig. 6. shows that the peaks are not sharp, indicates that the filters are amorphous. This demonstrates that adding cocoa shells activated charcoal filler to the filter does not increase the intensity.
3.7. Ammonium absorption analysis
The absorption test of ammonium in greywater with chacteristic as presented in Table 1, with various filter compositions for 1 hour adsorption time is shown in Table 2. The results showed that the filter with a composition of (75:25)% was the most effective filter for absorbing ammonium in greywater, with the absorption process
successfully reducing the concentration of gray water from 33.64 ppm to 10.68 ppm and a removal efficiency of 68.25%. These findings are consistent with physical test data for porosity and water absorption, which show that a 75:25 ratio is the best filter composition.
4. Conclusion
Filter based on zeolite-activated charcoal of cocoa shells has been successfully carried out. The results of characterization on various var- iations of filters show that the best physical test is found in the filter with a composition of (75:25)% which is sintered at a temperature of 700 ◦C with a porosity value of 53.01% and a water absorption capacity of 53.10%. Meanwhile, the filter with the best hardness value was the filter with a composition of (100:0)%, a sintering temperature of 900 ◦C, and a hardness value of 351.31 MPa. The ammonium absorber test results showed that the zeolite-activated charcoal filter of cocoa shells with a composition of (75:25)% was able to reduce the concentration of ammonium in greywater up to 68.25%.
Declaration of Competing Interest
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgement
The authors would like to express their gratitude to TALENTA Uni- versitas Sumatera Utara for funding the entire completion of this research with contract number 6789/UN5.1.R/PPM/2021 on June 16, 2021.
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Table 1
Characteristic of raw greywater.
No Parameter Unit Result
1 Ammonia-Nitrogen (NH3–N) mg/L 62.61
2 Nitrate mg/L <1.0
3 Total Phosphate as P mg/L 4
4 Smell – Stink
5 Detergent mg/L 138
Table 2
Ammonium adsorption capability of filters (n =5).
No. Sample/ (Filter with a variation composition of) Concentration (ppm)
1. Greywater 33.64 ±1.89
2. 100:0 20.16 ±2.01
3. 95:5 11.04 ±0.89
4. 90:10 16.16 ±2.74
5. 85:15 12.96 ±1.45
6. 80:20 14.68 ±1.63
7. 75:25 10.68 ±0.99
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